Preparation of synthetic organic detergent particles having only slight dust-forming tendencies



Patented July 8, 1947 PREPARATION OF SYNTHETIC ORGANIC DETERGENTPARTICLES HAVING ONLY SLIGHT DUST-FORNIING TENDENCIES Robert FranklinHeald, Nutley, and Minor Leslie 1- Givan, East Orange, N. 3., assignorsto Colgate- Palmolive-Peet Company, Jersey City, N. 3., a corporation ofDelaware No Drawing. Original application April 1'1, 1941,

Serial No. 388,989. Divided and this applicaf tion September 28, 1943,Serial No. 50%,160

4 Claims.

1 t The present invention relates to a process of treating syntheticdetergents and, more particularly, to a processor preparingwater-soluble non-fatty acid soap organic detergents, espe particles ofa synthetic detergent having greatly reduced dust-forming tendencies.

The invention further provides beads and grains of synthetic detergentsof the type of orcially those of the type of organic sulphates and 5genie ulp ates a d sul t having high sulphonates, in sprayed, granulatedand chip wasmng emciency and atlmosit only slight dustform to reducedust therein, and to the product formmg tendencies' f such process.Other objects and advantages of the present spray dried detergents havebeen employed for invention will be apparent to those skilled in theboth industrial and domestic uses for many years, art from the followingdescription because of their relative ease of solution due to Broadlystated according to the present inventhe large surface area exposedDetergents in tron, the addition of a relatively small proportion chipand granulated form have Similarly been of a petroleum 011 fraction to asynthetic deterused for the ,same reason; Up to the advent of gentresults in a composition having considerably the present invention therewere attendant less tendency to form dust. Aremarkable featureadvantages in the use of these materials which of the invention is thatthe addition of the oil considerably limited their employment. Becausehas httle or no effect upon the washing emclency' of their reduced size,there is always associated The incorporatior. of mineral on isparticuwith the product an appreciable portion of fines, larlyadvantageous m the ufacture of spray which causes a dust nuisance. Thisdust is 0bgranulated and chip detergents of the type of jectionable bothfrom the standpoint of cleanliorgan? sulpgateiapd g f g g ness andbecause it acts as an irritant upon the of ad mg t e 01 m ng e proveemucous membrane of the usen tergent beads and grains of the inventioncom- In seeking a method for eliminating these dispnses sp-mying thedetergent m fluid liquid advantages, the prior art has suggestedreducing or plastic) form into an air stream in a tower the proportionof fines. This was, at best an in a procedure commonly employed in theart expensive operation, and it was found, moreover, 3 g'g gg fg E thatthe removal of fines in any practical degree g a 0 mg c a er 1 e usua me en spraying oil upon the detergent particles had little efiect uponthe amount of dust raised during the cooling operation This method of inthe use of these synthetic detergent particles. ti th mi 1 i1 1 1 Thiswas due to the fact that the most troublei g 1 g? 2 y E as a so some orirritating dust is produced by the disin- 32 23 13 2.923? g g fi g ai 2:2: 3 irsleagggfiign of ti}? coarser pariztmlles durmg no granulation Ofa mechanical mixture of detergent m mg m a par mu any fi! 1e P 35 chipsor flakes and dry builders. In general, in g sma Percentage but VeryobJf'ctlonable the manufacture of synthetic detergent products 533 g igfigiz g gg gfi g ii zfi i fi' other than mechanical mixes, the mineraloil may be added in bulk to the detergent material .0 it i moreconvenien us, t e a i ion of the known, has given a satisfactorysolution upon a eral oil to the crutcher mix requires no greater i l? 212 b co t: i grz zfi invention to pro 5 it and, in general, also yieldsSatisac ory resu s. vide an improved process for treating synthetic Thepresent process is applicable to the treatt t uring the manufacture ofsaid dement of various water-soluble, non-fatty acid tergents in spr yeranul t d nd hip f rm soap, organic detergents, such as the salts of toreduce dust therein, whereby detergent parorganic sulphates andsulphonates, with or withticles having grgatly reduced irritant efiectin out any of the builders or fillers usually employed use are pr uce bythe art. A preferred roduct com rises the It is also an object of thisinvention to provide sodium salt of sulphated coconut oil ?atty acid aprocess for preparing detergents of the type monoglyceride as the activeingredient. Other of organic sulphates andsulphonates inparticudetergents suitable for treatment include salts late form havingonly slight dust-forming tendof sulphonated and sulphated long-chainfatty encies. alcohols. Thus, mineral oil can be added in Another objectof the invention is to provid any of the manners described to syntheticdetertions.

gents containing the sulphuric esters of oleyl alcohol, of laurylalcohol or of primary stearyl alcohol, salts thereof, including sodiumlauryl sulphate or the like, etc., to produce our novel compositions andto achieve the desirable results pertaining thereto and hereindescribed.

In selecting a. petroleum fraction for use in accordance with theinvention, kerosene (astral 011), white mineral oil, and heavy mineraloils of various viscosities are especially suitable for reducingdust-forming tendencies when incorporated in the detergent. Of these,the higher fractions are somewhat more desirable in that smallerproportions of the oil can be used and that there is less odor.Specifications for suitable oils are as follows:

Kerosene A. P. I. gravity 46.0 Flash point F. 127 Initial boiling pointF.. 350 Final dr p TL. 536

' White mineral oil Specific gravity, 15.6 0.845 to 0.855 ViscositySaybolt, 100 F sec 80 to 90 Initial boiling point F 572 90% distilled atF 748 Residue per cent 10 Heaoy mineral oils N o. 1 No. 2 N0. 3

300 365 ass Initial boiling point, "n... 568 609 597 Final distillationpoint, F 754 737 711 Distilled, percent 95 80 40 Residue, percent 5 2060 Still higher boiling fractions, having Saybolt viscosities of morethan 600 seconds, give very satisfactory results. Q

It is advantageous to employ oils with flash points high enough to avoidfire hazards, especially where the oil is incorporated in the detergentbefore spraying, as the high temperature of the spraying tower must betaken into consideration. In selecting the mineral oil, the viscosity ofthe oil is not of great efiect, although slightly better results areobtained with oils of higher viscosity. This may be due, in part, to thefact that these oil in general represent higher frac- If the oil is tooviscous, it is diflicult to handle and can therefore be inconvenient.

Using such oils as hereinbefore described, proportions of the mineraloil of about 0.5% to about 8.0% (on the basis of the finished product)reduce the dust-forming tendencies in synthetic detergent particles.When using oils of relatively high boiling fractions, about 0.5% toabout 3.0% of oil is suitable, about 0.5% to about 1.5% of m.'.1- eraloils of this type being preferred. This proportion decreases dust to aminimum, without affecting the detergent properties and handleability ofthe product. It will be understood that larger proportions of mineraloil must be employed where lighter fractions are used, and, in somecases, even several per cent, e. g., as much as about 2.5% to about 8%,are preferred for reducing dust to the considerable degree desired.Below the optimum proportion of mineral oil, of the preferred type, thebest results are not obtained, above this proportion, the treatedparticles exhibit a certain stickiness, which is undesirable from thestandpoints of both the consumer and the packager, and the detergencyvalue of the product is deleteriously affected.

The followin example is merely illustrative of the present invention,and it will be understood that the invention is not limited thereto.

Example About 0.65 part of a heavy mineral oil (mineral oil No. 3) isadded to 99.35 parts of an organic detergent solution in a crutcher. Thedetergent solution has the following composition, the active 1ingredient being the sodium salt of sulphated coconut oil fatty acidmonoglyceride:

I'he materials are thoroughly mixed, and the mixture is passed to aspray tower for spraying in a usual manner.

Upon spray drying, about 59.2% of the crutched material is lost asmoisture. The dried product gives the following analysis, the mineraloil showing up with any unreacted material:

Per cent Moisture About 1.0 Inorganic salts About 61.4 Active ingredientAbout 32.6 Unreacted (raw material) About 3.4 Mineral oil About 1.6

The results obtained according to the present invention are superior tothose obtained by the prior art. Even where part of the fines insynthetic detergent particles has been removed by sizing, the dustraised with such material is much greater than with the oil-treatedmaterial of this invention.

The term particle used in the present specification and in the appendedclaims is intended to include sizes and shapes of material having atleast one dimension of relatively low order, such as grains, beads,chips, flakes and other forms having proportionately large surface area.Similarly, the term particulate as applied to synthetic detergents isintended to include those forms having at least one small dimension.Particles having solid centres are usually referred to as grains, whilehollow particles are generally known as beads. Grains and beadsfrequently occur together and are distinguishable from chips and flakesin that all of their dimensions are of relatively low order.

The present application is a division of our prior application SerialNo. 388,989, filed April 17, 1941.

The present invention has been described with reference to illustrativeexamples and proportions, but it will be appreciated by those skilled inthe art that other variations and modifications of our invention can beemployed and that equivalents can be substituted therefor, withoutdeparting from the principles thereof.

We claim: 1. A process of preparing detergent particles which comprisesforming particles of a synthetic organic non-soap water-solubledetergent of the class consisting of sulphates and sulphonates, andspraying said particles after formation with an initial boiling pointabout 0.5% to about 3% of a mineral oil fraction having an initialboiling point of about 350 F., said percentage being based upon theamount of mineral oil in the final product, whereby improved particleshaving only slight dust-forming tendencies are produced.

2. A process of preparing detergent particles which comprises sprayingabout 0.5% to 8% of a mineral oil fraction havin an initial boilingpoint of at least about 350 F. upon preformed particles of a syntheticorganic non-soap watersoluble detergent of the class consisting ofsulphates and sulphonates, said percentage being based on the amount ofmineral oil in the final product, whereby particles having reduceddustforming tendencies are produced.

3. A process of preparing detergent particfes having only slightdust-forming tendencies which comprises mixing a mineral oil fractionhaving of at least about 350 F. with a synthetic organic non-soapwater-soluble detergent of the class consisting of sulphates andsulphonates in fluid form, and then forming said mixture into particles,the amount of said oil being within the range of about 0.5% to 8% byweight of said particles.

4. A process of preparing detergent particles having only slightdust-forming tendencies which comprises mixing a mineral oil fractionhaving an initial boiling point of at least about 350 F. with asynthetic organic non-soap water-soluble detergent of the classconsisting of sulphates and sulphonates, and then spray drying saidmixture, the amount of said mineral oil being within the range of about0.5% to 8% by weight of the spray dried product.

ROBERT FRANKLIN HEALD.

MINOR LESLIE GIVAN.

REFERENCES CITED The following references are of record in the file ofthis patent:

UNITED STATES PATENTS Number Name Date 1,715,999 Flammer et a1 June 4,1929 2,016,289 McGill Oct. 8, 1935 2,206,289 McDaniel July 2, 19402,130,362 Muncle Sept. 20, 1938 1,886,632 Broeman Nov. 8, 1982 1,479,757Trent Jan, 1, 1924 2,296,121 Smith Sept. 15, 1942 2,356,443 BissingerAug. 22, 1944 FOREIGN PATENTS Number Country Date 23,054 Great Britain1894 447,521 Great Britain Dec. 28, 1937 OTHER REFERENCESDyestuffs-Booklet of Allied Chem. 8: Dye

Com, N. Y., Sept. 1942, page 205.

